Nanocrystalline NiFe 2 O 4 particles were prepared by conventional sol-gel, citrate-nitrate sol-gel combustion and coprecipitation methods. The synthesized samples were annealed at 1000°C for two hours and structural, chemical, morphological, optical and magnetic properties of nickel ferrite were investigated. The structural properties were investigated by X-ray diffraction (XRD) technique which confirmed the formation of single phase NiFe 2 O 4 particles derived by the three methods. The chemical properties were analyzed by Fourier transform infrared (FT-IR) spectroscopy which confirmed the corresponding vibration modes in the samples. The optical properties were studied by UV-Vis spectroscopy. The morphological study of the as-synthesized samples was carried out by scanning electron microscopy (SEM). SEM images showed the agglomerated nanoparticles of NiFe 2 O 4 . The magnetic properties were investigated by vibrating sample magnetometer (VSM), which showed that the calcined samples exhibited typical magnetic behavior.